Abstract: The synthetic reaction of HDI biuret polyisocyanate was monitored by gel permeation chromatography (GPC). The best reaction process was selected according to the percent age of HDI biuret, and the influence of operation conditions on product was also analysed. The results demonstrated that the method of using steam with hexamethylene diisocyanate (HDI) monomer is the best process.Reaction temperature is controlled at 120?℃ and reaction time is controlled at about 7 hours.